A novel visible light active TiO/FeS semiconductor photocatalyst was synthesized by a simple wet chemical process. X-ray diffraction (XRD) was used to analyze the anatase TiO and pyrite structures in FeS/TiO nanocrystals. Scanning electron microscopy (SEM) confirmed the spherical morphology of composite nanocrystals. X-ray photoelectron spectroscopy (XPS) identified the Fe, S, Ti, and O oxidation states of relevant species. Energy dispersive X-ray (EDX) analysis was performed for compositional analysis. The measured band gap of the TiO/FeS nanocomposite system was 2.67 eV, which is smaller than un-doped TiO (3.10 eV) and larger than FeS (1.94 eV). The photocatalytic activity of TiO/FeS was significantly higher than pure FeS for degrading methylene blue (MB) under solar light irradiation due to the increase in visible light absorption, reduction in band gap energy, and better election-hole pair separation. The photocatalytic degradation of MB was investigated under the influence of solution pH, dye concentrations, and varied catalyst dosage. The optimum degradation (100%) of MB was observed in 180 min and the photocatalysis of MB reduced as the dye concentrations in the solution increased from 15 to 75 mg L. These results prove that the TiO/FeS nanocomposite has the stability, recycling, and adaptability for its practical application as a visible light photocatalyst for wastewater treatment. TiO/FeS showed increased degradation of the organic pollutant; which is confirmed by the increased rate of chemical reaction following pseudo first-order reaction kinetics with the highest rate constant value of 0.0408 m having highest value of 0.9981.